Glue composition containing vetch seed meal



Patented Oct. 12, 1948 GLUE COMPOSITION CONTAINING VETCH SEED MEAL Gustave Widmer, Basel, and Wilhelm Hertner,

Pratteln, Switzerland, assignors to Ciba Lim ited, Basel, Switzerland, a Swiss firm No Drawing. Application April 24, 1945, Serial No. 590,125. In Switzerland May 16, 1944 3 Claims. (Cl. 260-6) The present invention is concerned with an extender for glue consisting substantially of pure vetch meal in a state of very fine subdivision. It comprises the extender itself as well as glue compositions containing the same, and their use in the industry.

It is known that the vetch seeds, which are obtained in the refining of cereal grain, and which are generally admixed with larger or smaller quantities of the seed of other weed plants, such as campion, lathyrus, wild mustard and cow-wheat, can be used in the ground state as an extender for natural or artificial glues. Owing to the difilculty of disintegrating the hard husk constituents, the commercial vetch meal obtained in the usual manner generally consists of a. mixture of finely divided pale yellow meal of the kernel and coarser husk constituents of darker colour.

It has now been found that the usefulness of this commercial vetch meal as an extender for glues isvery limited. Although in the case of low degrees of dilution, for example, ranging from 30 to 100 per cent, such as are sufficient in practice with inexpensive natural glues such, for example, as casein glue, no considerable deterioration of the glue can be detected,-the impairment becomes very marked at greater degrees of dilution, for example, amounting to about 2-3 times the weight of theglue, such as are desired in the interests of economy with the expensive artificial resin glues. The tenacity of the glue bond in the dry state i usually adequate or good even with large additions of commercial vetch meal, for example, when 300 parts of vetch meal are used with 100 parts of urea resin glue. On the other hand, the tenacities of the bonds in wet condition (wet tenacity) show widely divergent values, that is to say, in addition to strengths which are satisfactory some have been observed which are entirely useless, and the reason for this extraordinary behaviour has not been determined heretofore. Consequently the value of commercial vetch meal as an extender for artificial resin glues, especially urea resin glue, has

been open to question.

The present invention is based on the unexpected observation that by using sorted, pure vetch seeds a meal can be obtained which, when used as an extender for artificial resin glues, especially urea resin glues, does not lead to glue bonds exhibiting the above mentioned divergencies in wet tenacity.

Thus, it has been found the varying quantities of other seeds, especially campion seeds, present in the crude vetch seeds are largely responsible for the non-uniform properties of the glue bonds obtained when commercial vetch meal is used as an extender. In fact when the nieal of campion seeds is used alone a extender, glue bonds are obtained whose wet tenacities are lower than those of bonds obtained when pure vetch meal is used.

A further improvement can be secured by increasing the degrees 0! fineness oi the pure vetch meal. It has been found that as the degree of finenes is increased the values of wet tenacity approach those of the dry tenacity.

Increasing the degree of fineness of the vetch meal also has the advantage that no unusable husk residues remain and there is no need to use the paler colored fractions (kernel meal) separately, so that, if desired, a complete vetch meal can be produced without there being any waste material. For this purpose the husk constituents which are more diflicult to disintegrate may be separated by sifting during the disintegration, and separately disintegrated in a special mill, for example, a high speed hammer mill, and only mixed with the remainder of the vetch meal in the form of a very fine powder. In order to avoid unduly high temperatures which might be injurious to the protein content of the vetch meal it is of advantage, when working with high speed mills, to provide cooling means.

The invention therefore provide an extender for glues which is based on vetch meal, and which, as compared with the known glue extenders composed of vetch meal, is improved in two respects simultaneously, namely: freedom of the vetch seeds used from foreign seed material, especially campion seeds, and a greater degree of fineness of the pure vetch meal.

The improvement in the wet tenacity of the glue bonds obtained with the extender of the invention is especially surprising in the case of the thermosetting artificial resin glues based on urea-formaldehyde, which cannot be extended with the known extenders, for example, commercial vetch meal, to an extent greater than 50-100 per cent without the wet tenacity of the resulting glue bonds being considerably impaired. Thus, for example, more than 300 parts of pure vetch meal of the quality described above can be used tially freed, from foreign seed material, which meal has such a high degree of fineness that at least 65 per cent of it passes through a sieve of size VI (Pharm. Ifelv. V), that is to say, having a mesh of 0.17 millimetre (clear opening).

Example 1 A pure vetch meal (I) free from husk and obtained by the usual methods of milling was subjected to sieve analysis, and separated into fractions with the use of DIN-sieves Nos. 40, 50, '70 and 100, that is to say, of sieves having meshes of 0.15, 0.12, 0.088 and 0.060 millimetre (clear openings), respectively. The fractions so obtained were used as glue extenders in the following series of tests. 30 grams of each fraction were separately mixed with 10 grams of urea resin glue, 0.5 gram of urea and 0.5 gram of ammonium chloride in the dry state, and each mixture was treated with about 30 cc. of water and well stirred to form a spreadable glue. With th resulting glues beech veneers of 1.4 mm. thickness were glued together in a hot press to form plywood. The resulting plywood sheets were tested in known manner for dry tenacity after being allowed to stand under dry conditions for 4 days, and for wet tenacity after remaining in water at room temperature for 4 days.

The same series of tests was carried out with a pure vetch meal (11) obtained by the same methods but containing much husk material.

. The following results were obtained with the application of 300 grams of glue per squar metre of glued surface, and by hot pressing at a pressure of 10 kilograms per square centimetre with a plate temperature of 100 C. for a period of 5 minutes.

Tenacity in kilograms per square centimetre Fineness of the meal Veicl} meal vetcililmeal dry wet wet Retained on sieve No. 40 25.0 11.8 23. 2 4.1 Retained on sieve No. 50 B. 2 11.3 27. 6 11. 3 Retained on sieve No. 70-... 32. 9 15. 2 29. 12. 6 Retained on sieve No. 100 29. 5 15. 6 28. 6 12. 9 Through sieve No. 100 28.8 15.0 28. 5 l3. 2

It will be seen from the above figures that a coarse state of division leads to a considerable reduction in wet tenacity especially in the case dehyde in neutral aqueous solution at about C. in a closed vessel until a cooled test portion gives a strong precipitation when diluted with water. The solution is then dried with care, and the residue is pulverised.

Exam le 2 Vetch seed material obtained in the refinin of cereal grain ,was freed in known manner from foreign seed material especially campion seeds. During the process of disintegration the husk and kernel portions were separated from one another by sifting, andeach portion was separately further disintegrated to a fine powder. a high speed hammer mill being used for disintegrating the husk portions. When the fine disintegration was complete the two portions were mixed together, and the pure complete vetch meal so obtained was used as an extender for urea resin glue, in the following series of tests.

The urea resin glue was the same as the product used in Example 1. The extender was added to the glue in quantities ranging from 0-500 per cent. As hardening agent there were again used f the test procedures described in Example 1 and the following results were obtained;

Tenacity in kilograms Pure vetch per square centimetre meal addition 7 dry wet Per cent 1 0 32. 4 28. 4 25 34.9 29. 5 50 35. 3 25. 6 mo 34. 3 23. l 33. 0 23. 8 32. 7 25. 2 33. 2 2i. 2 mo 31. 8 21. 6 225 31. 2 l9. 4 250 33. 3 17. 6 275 32. 2 so. 8 300 35. 3 l7. 8. 325 32. 4 17. 7 350 31.5 1L6 375 30. 1 l8. 6 400 30. 0 17,9 425 28. 5 l3. 7 450 26. 3 l2. 6 475 22. 5 l3. 8 500 28. 8 l4. 8

Instead of the urea resin glue mentioned in Example 1, other carbamide resin glues can be used with similar success.

Example 3 Vetch seed material was freed from foreign seed material in known manner, and finely disintegrated; The husk portions were very finely pulverised in a high speed hammer mill and the remainder of the vetch meal was mixed therewith. In like manner campion seeds were finely disintegrated, and a campion meal produced therefrom. In order to ascertain the effect of the two kinds of meal on the wet tenacity a series of tests were carried out using the two said meals and mixtures thereof together with the urea resin mentioned in Example 1. 1 The glueing and test conditions were the same as in Example 1, namely: about 300 grams of glue per square metre of glued surface, a glueing pressure of 10 kilograms ,per square centimetre, a glueing temperature of 100 C., and a pressing time of '5 minutes. The proportion of extender used amounted to 300 per cent, that is to say, 300 parts of extender per 100 parts of urea resin glue were used. 1

Thus, while the use of pure vetch meal leads to glue bonds which even with 300 per cent of extender can be regarded as very resistant to cold water, even small additions of campion meal lead to a reduction of this value, which does not substantially or with certainty fulfil the requirements for water resistant, glued ply sheets (15 kilogram per square centimetre).

Example 4 During the disintegration of pure vetch meal there were withdrawn a very pale fraction of kernel meal as well as the coarsest husk portions, and the middle fraction containing a fairly large amount of husk material was disintegrated to a state of fineness almost imperceptible to the touch. Glueing operations were carried out with a melamine formaldehyde resin with the addition of increasing quantities of the above mentioned extender, the conditions being the same as those described in Example 1 with the use of beech wood veneers of 1.4 mm. thickness. The following results were obtained with an application of 300 grams of glue per square metre of glued surface, and under a pressure of 10 kilograms per square centimetre at a plate temperature of 100 C. and a pressing'time of 15 minutes.

Tenacity in kilograms per square centimetre Parts of ex- Breakdown alter tender r l00 Dry Brea'x- Wet Breakremaining for 1 parts 0 meladown down hour in water mine resin at 100 0.

l 20 I 15 I 10 0 100 30. 4 22. 1 15. 6 {25 29. 3 24. 1 l3. 7 30. 8 28. 7 l3. 2 17 34. 0 29. 6 15. 0 200 33. 5 28. 7 l2. 6 225 33. 3 28.8 18.6 $0 36. 4 28. 8 13. 2 275 33. 2 2i. 2 12. 2 I 300 34. 1 2o. 6 delaminated 350 38. 6 Z). 8 deluninated 400 N. 3 l8. 6 delam lnatcd 450 34. 1 l8. 8 dellminnted 500 35. 2 17. 1 delaminatnd 1 Requirement for water-proof plywood.

The figures clearly show that with the extender used the wet tenacity and resistance to boiling water are maintained to a quite surprising extent even with large quantities of extender.

The melamine formaldehyde resin used in the foregoing example may, for example, be prepared by condensing one mol of melamine with 3 mols of aqueous formaldehyde in a weakly basic solution at 80 C. until a test portion gives a strong precipitation when diluted with a little water. The resin solution is then carefully dried, and if desired disintegrated.

What we claim is:

1. A glue composition containing athermosetting synthetic resin of the group consisting of urea-formaldehyde resin and melamine-formaldehyde resin and also containing as an extender a meal from vetch seeds substantially freed from foreign seed material, which meal has such a high degree of fineness that at least per cent of it passes through a sieve having a mesh of at the most 0.17 millimetre (clear opening) 2. A glue composition containing a thermosetting synthetic resin of the group consisting of urea-formaldehyde resin and melamine-formaldehyde resin and also containing as an extender a meal from vetch seeds substantially freed from foreign seed material, which meal includes the whole husk portion and has such a high degree of fineness that at least 65 per cent of it passes through a sieve having a mesh ofat the most 0.17 millimetre (clear opening).

3. A glue composition containing a thermosetting synthetic resin of the group consisting of urea-formaldehyde resin and melamine-formaldehyde resin and also containing as an extender a husk-free fraction of a meal from vetch seeds substantially freed from foreign seed material, which meal has such a high degree of fineness that at least 65 percent of it passes through a sieve having a mesh of at the most 0.17 millimetre (clear opening) GUSTAVE WIDll/llllR. WEI-ELM HERTNER.

No references cited. 

